KR950031895A - Advanced Oxidation of Organic Chemicals - Google Patents

Advanced Oxidation of Organic Chemicals Download PDF

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KR950031895A
KR950031895A KR1019950011370A KR19950011370A KR950031895A KR 950031895 A KR950031895 A KR 950031895A KR 1019950011370 A KR1019950011370 A KR 1019950011370A KR 19950011370 A KR19950011370 A KR 19950011370A KR 950031895 A KR950031895 A KR 950031895A
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oxygen
impeller means
liquid
gas phase
hollow
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KR100238501B1 (en
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폴 킹슬리 제프리
캐더린 로비 앤
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조안 엠. 젤사
프랙스에어 테크놀로지, 인코포레이티드
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01F23/23761—Aerating, i.e. introducing oxygen containing gas in liquids
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    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/92—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with helices or screws
    • B01F27/921—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with helices or screws with helices centrally mounted in the receptacle
    • B01F27/9211—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with helices or screws with helices centrally mounted in the receptacle the helices being surrounded by a guiding tube
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    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/1868—Stationary reactors having moving elements inside resulting in a loop-type movement
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
    • C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
    • C07C51/255—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting
    • C07C51/265—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting having alkyl side chains which are oxidised to carboxyl groups
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    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
    • C07C63/14—Monocyclic dicarboxylic acids
    • C07C63/15—Monocyclic dicarboxylic acids all carboxyl groups bound to carbon atoms of the six-membered aromatic ring
    • C07C63/26—1,4 - Benzenedicarboxylic acid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01F23/233—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids using driven stirrers with completely immersed stirring elements
    • B01F23/2336—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids using driven stirrers with completely immersed stirring elements characterised by the location of the place of introduction of the gas relative to the stirrer
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    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05—Stirrers
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    • B01F27/114—Helically shaped stirrers, i.e. stirrers comprising a helically shaped band or helically shaped band sections
    • B01F27/1144—Helically shaped stirrers, i.e. stirrers comprising a helically shaped band or helically shaped band sections with a plurality of blades following a helical path on a shaft or a blade support
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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
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Abstract

본 발명은 순산소 및 거의 순산소를 사용하고 증발성 냉각을 이용하여 수행되는 유기 화학물질 산화반응에 관한 것이다. 이에 의해 유용한 조작이 달성되고, 고체 생성물 또는 부생성물의 생성을 야기시키는 유기 화학물질의 산화는 고체 생성물 또는 부생성물로 피복되게 되는 직접 접촉 열교환 표면에 대한 필요성을 제거함으로써 촉진된다.The present invention relates to organic chemical oxidation reactions carried out using pure oxygen and near pure oxygen and using evaporative cooling. A useful operation is thereby achieved, and the oxidation of the organic chemicals causing the production of solid products or byproducts is facilitated by eliminating the need for a direct contact heat exchange surface to be covered with the solid product or byproducts.

Description

향상된 유기 화학물질의 산화방법Advanced Oxidation of Organic Chemicals

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음As this is a public information case, the full text was not included.

제2도는 본 발명의 한 구현을 나타내는 LOR 혼합용기의 개략적 측면도.2 is a schematic side view of a LOR mixing vessel showing one embodiment of the present invention.

Claims (18)

(a) 유기 용매중에 존재하는 산화시키려는 유기 화학물질을 함유하고, 천정 기체상과의 기체-액체 계면을 갖는 반응 용기내에 함유된 액체부분을 그 안에 위치한 임펠러 수단에 의해 재순환 흐름 패턴으로 유지시키는 단계; (b)상기 임펠러 수단에 의해 생성된 난류 영역내에 있을 정도로 상기 임펠러수단 근처의 산소 주입지점(들)에서 액체부분의 상기 재순환 부분내로 순산소 또는 산소-부화 기체를 직접 주입시켜서, 액체 내로의 주입시에 빠른 소모를 위해 작은 기포로서 액체중의 산소를 빠르게 분산시키는 단계(유기 화학물질의 산화로 인한 반응열은 상기 액체 영역중에 존재하는 휘발성 유기 재료 및 물의 증발시에 증발성 냉각에 의해 제거되고, 단지 소량의 산소에 의해 달성된 상기 증발된 유기 재료-및 수증기의 기포는 상기 액체부분 중에서 그리고 반응 용기의 상부중의 비교적 부통의 비-난류 영역을 통해 기체-액체 계면 및 상기 천정 기체상까지 상상하며, 상기 반응 용기는 직접 접촉 기계적 냉각 수단을 함유하지 않음); 및 (c)상기 증발된 유기 재료 및 수증기의 기포를 천정 기체상으로 부터 배기시켜서, 산소 및 산화시키려는 유기 화학물질을 산소의 빠른 소모 및 천정 기제상으로 통과되는 최소량의 산소기포에 의한 유기 재료 및 물의 증발을 조장하는 조건하에서 혼합시키는 단계로 이루어진, 천정 기체상에 대한 산소의 현저한 손실없이, 반응 용기내에 함유된 액체부분에 존재하는 유기화학물질을 산화시키는 방법.(a) maintaining a liquid portion contained in a reaction vessel containing an organic chemical to be oxidized in an organic solvent and having a gas-liquid interface with a ceiling gas phase in a recycle flow pattern by means of impeller means located therein; ; (b) injecting pure oxygen or oxygen-enriched gas directly into the recycle portion of the liquid portion at the oxygen injection point (s) near the impeller means to be within the turbulent region produced by the impeller means, thereby injecting it into the liquid Rapidly dispersing oxygen in the liquid as small bubbles for rapid consumption at the time (heat of reaction due to oxidation of organic chemicals is removed by evaporative cooling upon evaporation of volatile organic materials and water present in the liquid region, Bubbles of the evaporated organic material and water vapor achieved by only a small amount of oxygen are envisaged to the gas-liquid interface and the ceiling gas phase through the relatively non-turbulent region in the liquid portion and in the top of the reaction vessel. The reaction vessel does not contain direct contact mechanical cooling means); And (c) evacuating the evaporated organic material and water vapor bubbles from the ceiling gas phase, so that the oxygen and the organic chemicals to be oxidized are rapidly consumed by oxygen and the organic material by the minimum amount of oxygen bubbles passed through the ceiling substrate, and A method of oxidizing an organic chemical present in a liquid portion contained in a reaction vessel, without significant loss of oxygen to the ceiling gas phase, comprising mixing under conditions that promote evaporation of water. 제1항에 있어서, 비활성 기체를 천정 기체상을 통해 통과시켜서, 천정 기체상을 통과하는 소량의 산소를 비활성화시키는 단계를 더 포함함을 특징으로 하는 방법.The method of claim 1 further comprising passing an inert gas through the ceiling gas phase to deactivate a small amount of oxygen passing through the ceiling gas phase. 제1항에 있어서, 재순환 액체 흐름 패턴을 반응용기의 하반부에 위치한 축방향 흐름 하향 펌핑 임펠러수단에 의해 액체 영역중에 유지시키며, 임펠러 수단에 의해 생성된 상기 난류 영역중에 순산소 또는 산소-부화 기체의 주입지점이 있고, 상기 임펠러 수단은 임펠러 수단을 통과하는 액체내로 구독축을 따라 천정 기체상으로 부터의 기체의 흡입을 방지하도록 상향으로 연장한 구동축 및 그 위에 위치한 배플수단을 갖고, 용해되지 않은 산소를 트랩핑시키고 이것의 용해를 향상시키는 고난류 고울셀을 생성시키도록 고속으로 액체가 상기 하향 펌핑 임펠러 수단을 통과함을 특징으로 하는 방법.The method of claim 1, wherein the recirculating liquid flow pattern is maintained in the liquid region by an axial flow downward pumping impeller means located in the lower half of the reaction vessel, and wherein There is an injection point, the impeller means having a drive shaft extending upwards to prevent the intake of gas from the ceiling gas phase along the subscription axis into the liquid passing through the impeller means and a baffle means positioned thereon, for dissolving undissolved oxygen Wherein liquid flows through said downward pumping impeller means at high speed to produce a high turbulence goulcell that traps and enhances its dissolution. 제3항에 있어서, 상단 및 바닥에서 개방단부를 갖는 중심에 위치한 중공 통풍관의 하부에 축방향 흐름 하향 펌핑 임펠러 수단이 위치하며, 액체의 재순환 흐름이 중공 통풍관 내에서 하향으로 그리고 그 외측에서 상향으로 흐르게 되며, 중공 통풍관은 이것의 바닥부분의 길이의 0 내지 200%의 수직거리로 상향으로 연장한 확대된 원뿔형으로 벌어진 상부를 갖고, 상기 상부는 상기 중공 통풍관의 상단을 가로지르는 액체의 하향 속도를 최소화시키는 확대된 상부직경을 가짐을 특징으로 하는 방법.4. A pump according to claim 3, wherein an axial flow downward pumping impeller means is located at the bottom of the centrally located hollow vent with open ends at the top and bottom, wherein the recirculating flow of liquid is downwards and outwards in the hollow vent. Which flows upwards, the hollow ventilating tube has an enlarged conical top that extends upwards at a vertical distance of 0 to 200% of the length of its bottom portion, the upper portion of the liquid traversing the top of the hollow ventilating tube. Characterized in that it has an enlarged upper diameter to minimize the downward velocity of the. 제4항에 있어서, 산소 주입 지점이 상기 축방향 흐름 하향 펌핑 임펠러 수단 아래의 중공 통풍관 내에 있음을 특징으로 하는 방법.5. A method according to claim 4, wherein the oxygen injection point is in a hollow vent below the axial flow downward pumping impeller means. 제5항에 있어서, 방사형 흐름 임펠러 수단이 상기 축방향 하향 펌핑 임펠러수단 아래의 상기 중공 통풍관내에 위치하고, 상기 산소 주입지점이 축방향 흐름 하향 펌핑 임펠러 수단과 상기 방사형 흐름 임펠러 수단 사이에 위치함을 특징으로 하는 방법.6. A radial flow impeller means according to claim 5, wherein a radial flow impeller means is located in the hollow vent below the axial downward pumping impeller means and the oxygen injection point is located between the axial flow downward pumping impeller means and the radial flow impeller means. How to feature. 제5항에 있어서, 방사형 흐름 임펠러 수단이 상기 하향 펌핑 임펠러 수단 아래의 상기 중공 통풍관내에 위치하고, 상기 산소 주입 지점이 상기 방사형 흐름 임펠러 수단아래에 위치함을 특징으로 하는 방법.6. A method according to claim 5, wherein radial flow impeller means are located in the hollow vent below the downward pumping impeller means and the oxygen injection point is located below the radial flow impeller means. 제4항에 있어서, 산소 주입 지점이 중공 통풍관 아래에 있음을 특징으로 하는 방법.5. The method of claim 4 wherein the oxygen injection point is below the hollow vent. 제2항에 있어서, 상기 액체 부분이 약간 과량의 기체 산소가 존재하는 반응 혼합물의 비점에서 유지됨을 특징으로 하는 방법.The method of claim 2, wherein the liquid portion is maintained at the boiling point of the reaction mixture in which a slight excess of gaseous oxygen is present. 제4항에 있어서, 중공 통풍관의 원뿔형으로 벌어진 상부가 이것의 바닥 부분의 길이의 100% 내지 150%까지 상향으로 연장됨을 특징으로 하는 방법.5. A method according to claim 4, wherein the conical flared top of the hollow vent extends upwardly from 100% to 150% of the length of its bottom portion. (a) 유기 용매 중에 존재하는 산화시키려는 유기 화학물질을 함유하고, 천정 기체상과의 기체-액체 계면을 갖는 액체 부분을 함유하기 위한 반응용기(반응용기는 직접 접촉 기계적 냉각 수단을 함유하지 않은) (b) 반응 용기내에 액체 재순환 흐름 패턴을 유지시키기 위한 임펠러 수단; (c)상기 임펠러 수단에 의해 생성된 난류 영역내에 있을 정도로 상기 임펠러 수단 근처의 산소 주입 지점에서 액체 부분내로 순산소 또는 산소-부화 기체를 직접 주입시켜서, 액체 내로의 주입시에 빠른 소모를 위해 작은 기포로서 액체중의 산소를 빠르게 분산시키기 위한 주입 수단(유기 화학물질의 산화로 인한 반응열을 상기 액체 영역중에 존재하는 휘발성 유기 재료 및 물의 증발시에 증발성 냉각에 의해 제거되고, 단지 소량의 산소에 의해 달성된 상기 증발된 유기 재료-및 수증기의 기포는 상기 액체 부분 중에서 그리고 반응 용기의 상부중의 비교적 부동의 비-난류 영역을 통해 기체-액체 계면 및 상기 천정 기체상까지 상승함; 및 (d) 상기 증발된 유기재료 및 수증기의 기포를 천정 기체상으로 부터배기시켜서, 산소 및 산화시키려는 유기 화학물질을 산소의 빠른 소모 및 천정 기체상에 통과되는 최소량의 산소 기포에 의한 유기 재료 및 물의 증발을 조장하는 조건하에서 혼합시킬 수 있는 배기 수단으로 이루어진, 천정 기체상에 대한 산소의 현저한 손실없이, 반응 용기내에 함유된 액체 부분에 존재하는 유기 화학물질을 산화시키기 위한 시스템(a) a reaction vessel containing an organic chemical to be oxidized in an organic solvent and containing a liquid portion having a gas-liquid interface with the ceiling gas phase (the reaction vessel does not contain direct contact mechanical cooling means) (b) impeller means for maintaining a liquid recycle flow pattern in the reaction vessel; (c) injecting pure oxygen or oxygen-enriched gas directly into the liquid portion at an oxygen injection point near the impeller means to be within the turbulent region produced by the impeller means, thereby reducing the need for rapid consumption upon injection into the liquid. Injection means for rapidly dispersing oxygen in the liquid as bubbles (heat of reaction due to oxidation of organic chemicals is removed by evaporative cooling upon evaporation of volatile organic materials and water present in the liquid zone, and only in a small amount of oxygen Bubbles of the evaporated organic material- and water vapor achieved by rising to the gas-liquid interface and the ceiling gas phase through the relatively floating non-turbulent region in the liquid portion and in the top of the reaction vessel; and (d ) The organic chemicals to be oxygen and oxidized by exhausting the vaporized organic material and water vapor bubbles from the ceiling gas phase Reaction without significant loss of oxygen to the ceiling gas phase, consisting of exhaust means capable of mixing the vagina under conditions that facilitate rapid consumption of oxygen and evaporation of water and organic materials by the least amount of oxygen bubbles passing through the ceiling gas phase. System for oxidizing organic chemicals present in the liquid portion contained in the container 제11항에 있어서, 비활성 기체를 천정 기체상을 통해 통과시키기 위한 도관 수단을 포함함을 특징으로 하는 시스템.12. The system of claim 11, comprising conduit means for passing an inert gas through the ceiling gas phase. 제11항에 있어서, 상기 임펠러 수단은 반응용기에 위치한 축방향 흐름 하향 펌핑 임펠러 수단으로 이루어지며, 임펠러 수단을 통과하는 액체 내로 구동축을 따라 천정 기체상으로 부터의 기체의 흡입을 방지하도록 상향으로 연장한 구동축 및 그 위에 위치한 배플수단을 포함하고, 상기 하향 펌핑 임펠러 수단은 용해되지 않은 산소를 트랩핑시키고 이것의 용해를 향상시키는 고난류 로울 셀을 생성시키도록 고속으로 액체를 하향 펌핑시킬 수 있음을 특징으로 하는 방법.12. The method of claim 11, wherein the impeller means consists of an axial flow downward pumping impeller means located in the reaction vessel and extends upward to prevent intake of gas from the ceiling gas phase along the drive shaft into the liquid passing through the impeller means. A drive shaft and a baffle means located thereon, said downward pumping impeller means being capable of pumping liquid downward at high speed to produce highly turbulent roll cells that trap undissolved oxygen and improve its dissolution. How to feature. 제13항에 있어서, 상기 축방향 하향 펌핑 임펠러 수단이 위치한 중심에 위치한 중공 통풍관을 포함하며, 상기 중공 통풍관은 상단 및 바닥에서 개방단부를 가져서, 액체의 재순환 흐름이 중공 통풍관 내에서 하향으로 그리고 외측에서 상향으로 흐르게 되며, 중공 통풍관은 이것의 바닥부분의 길이의 0 내지 200%의 수직거리로 상향으로 연장한 확대된 원뿔형으로 벌어진 상부를 갖고, 상기 상부는 상기 중공 통풍관의 상단을 가로지르는 액체의 하향 속도를 최소화시키는 확대된 상부 직경을 가짐을 특징으로 하는 시스템.14. A hollow vent according to claim 13, comprising a hollow vent located at the center of which the axial downward pumping impeller means is located, the hollow vent having open ends at the top and the bottom, such that the recycle stream of liquid is downward in the hollow vent. Inwardly and outwardly, the hollow ventilated tube has an enlarged conical widened top extending upwardly at a vertical distance of 0 to 200% of its bottom portion, the upper end of which is the top of the hollow ventilated tube. And have an enlarged upper diameter that minimizes the downward velocity of the liquid across it. 제14항에 있어서, 산소 주입 지점이 상기 축방향 흐름 하향 펌핑 임펠러 수단 아래의 중공 통풍관 내에 있음을 특징으로 하는 시스템.15. The system of claim 14, wherein an oxygen injection point is in the hollow vent below the axial flow downward pumping impeller means. 제15항에 있어서, 상기 축방향 하향 펌핑 임펠러 수단아래의 상기 중공 통풍관 내에 위치한 방사형 흐름 임펠러 수단을 포함하며, 상기 산소 주임 지점이 축방향 흐름 하향 펌핑 임펠러 수단과 상기 방사형 흐름 임펠러 수단 사이에 위치함을 특징으로 하는 시스템.16. The radial flow impeller means according to claim 15, comprising radial flow impeller means located within said hollow ventilating tube below said axial downward pumping impeller means, said oxygen filling point being located between said axial flow downward pumping impeller means and said radial flow impeller means. System. 제15항에 있어서, 상기 하향 펌핑 임펠러 수단 아래의 상기 중공 통풍관내에 위치한 방사형 흐름 임펠러 수단을 포함하며, 상기 산소 주입지점이 상기 방사형 흐름 임펠러 수단 아래에 위치함을 특징으로 하는 시스템.16. The system of claim 15, comprising radial flow impeller means located in the hollow vent below the downward pumping impeller means, wherein the oxygen injection point is located below the radial flow impeller means. 제14항에 있어서, 중공 통풍관의 원뿔형으로 벌어진 상부가 이것의 바닥 부분의 길이의 100% 내지 150%까지 상향으로 연장됨을 특징으로 하는 시스템.15. The system of claim 14, wherein the conical flared top of the hollow vent extends upwardly from 100% to 150% of the length of its bottom portion. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
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